ASTM D5968-06(2013)
(Test Method)Standard Test Method for Evaluation of Corrosiveness of Diesel Engine Oil at 121 °C
Standard Test Method for Evaluation of Corrosiveness of Diesel Engine Oil at 121 °C
SIGNIFICANCE AND USE
4.1 This test method is intended to simulate the corrosion process of non-ferrous metals in diesel lubricants. The corrosion process under investigation is that believed to be induced primarily by inappropriate lubricant chemistry rather than lubricant degradation or contamination. This test method has been found to correlate with an extensive fleet database containing corrosion-induced cam and bearing failures.
SCOPE
1.1 This test method is used to test diesel engine lubricants to determine their tendency to corrode various metals, specifically alloys of lead and copper commonly used in cam followers and bearings. Correlation with field experience has been established.4
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in 5.3.1, 6.6, 6.7, 6.8, 6.9, 6.10, 6.11, 7.1.1, 7.1.2, 7.1.5, and 7.4.1.
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Standards Content (Sample)
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Designation: D5968 − 06(Reapproved 2013)
Standard Test Method for
Evaluation of Corrosiveness of Diesel Engine Oil at 121 °C
This standard is issued under the fixed designation D5968; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
INTRODUCTION
The method described in this test method is based on the gas turbine lubricant corrosion and
oxidation test described in FederalTest Method Standard 791, Method 5308. Because this test method
relates to corrosion in diesel engines rather than in gas turbines, temperatures, metal coupons, and
certain parts of the test procedure were modified to be more appropriate for heavy duty diesel engines.
The method described in this test method can be used by any properly equipped laboratory, without
outside assistance. However, the ASTM Test Monitoring Center (TMC) provides reference oils and
an assessment of the test results obtained on those oils by the laboratory (see Annex A1). By these
means, the laboratory will know whether their use of the test method gives results statistically similar
to those obtained by other laboratories. Furthermore, various agencies require that a laboratory utilize
the TMC services in seeking qualification of oils against specifications. For example, the U.S. Army
imposes such a requirement in connection with several Army engine lubricating oil specifications.
Accordingly, this test method is written for use by laboratories that utilize the TMC services.
Laboratories that choose not to use those services may simply ignore those portions of the test method
that refer to the TMC.
This test method may be modified by means of Information Letters issued by theTMC. In addition,
the TMC may issue supplementary memoranda related to the method (see Annex A1). For other
information, refer to the research report on the Cummins Bench Corrosion Test.
1. Scope 1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 This test method is used to test diesel engine lubricants
responsibility of the user of this standard to establish appro-
to determine their tendency to corrode various metals, specifi-
priate safety and health practices and determine the applica-
cally alloys of lead and copper commonly used in cam
bility of regulatory limitations prior to use. Specific hazard
followers and bearings. Correlation with field experience has
statements are given in 5.3.1, 6.6, 6.7, 6.8, 6.9, 6.10, 6.11,
been established.
7.1.1, 7.1.2, 7.1.5, and 7.4.1.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
2. Referenced Documents
standard.
2.1 ASTM Standards:
D130 Test Method for Corrosiveness to Copper from Petro-
This test method is under the jurisdiction of ASTM Committee D02 on leum Products by Copper Strip Test
Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
D5185 Test Method for Multielement Determination of
Subcommittee D02.B0.02 on Heavy Duty Engine Oils.
Used and Unused Lubricating Oils and Base Oils by
Current edition approved Oct. 1, 2013. Published October 2013. Originally
Inductively Coupled Plasma Atomic Emission Spectrom-
approved in 1998. Last previous edition approved in 2006 as D5968 – 06. DOI:
10.1520/D5968-06R13.
etry (ICP-AES)
ASTM Test Monitoring Center, 6555 Penn Ave., Pittsburgh, PA 15206-4489.
E691 Practice for Conducting an Interlaboratory Study to
(http://www.astmtmc.cmu.edu/)
Determine the Precision of a Test Method
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1322. The research report and
this test method are supplemented by Information Letters and Memoranda issued by
theASTM Test Monitoring Center. This edition incorporates revisions contained in
all information letters through No. 05–1. Users of this test method shall contact the For referenced ASTM standards, visit the ASTM website, www.astm.org, or
ASTM Test Monitoring Center to obtain the most recent of these. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Wang, J. C., and Cusano, C. M., “Development ofABench Test to Detect Oils Standards volume information, refer to the standard’s Document Summary page on
Corrosive to Engine Components,” SAE Technical Paper No. 940790, 1994. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5968 − 06 (2013)
FIG. 2 Sample Tube Head
FIG. 1 Sample Tube
2.2 U.S. Federal Test Method Standards:
Federal Test Method Standard 791, Method 5308.7 Corro-
siveness and Oxidation Stability of Light Oils (Metal
Squares)
3. Summary of Test Method
3.1 Four metal coupons of copper, lead, tin, and phosphor
bronze are immersed in a measured amount of engine oil. The
oil,atanelevatedtemperature,isblownwithairforaperiodof
time. When the test is completed, the coupons and the stressed
oil are examined to detect corrosion.
3.2 An industrial reference oil is tested with each group of
tests to verify test acceptability.
4. Significance and Use
4.1 This test method is intended to simulate the corrosion
process of non-ferrous metals in diesel lubricants. The corro-
sion process under investigation is that believed to be induced
primarily by inappropriate lubricant chemistry rather than
lubricant degradation or contamination. This test method has
been found to correlate with an extensive fleet database
FIG. 3 Air Tube
containing corrosion-induced cam and bearing failures.
5. Apparatus
5.1.4 Thermocouple Tube, Fig. 4.
5.1.5 Condenser, Allihn Type, Fig. 5.
5.1 The main apparatus consists of the following items of
5.1.6 Assembled Apparatus, Fig. 6.
standard wall borosilicate glassware as shown in Figs. 1-6.
5.1.1 Main Sample Tube, Fig. 1.
5.2 Additional glassware items and assembly accessories
5.1.2 Sample Tube Head, Fig. 2.
needed are:
5.1.3 Air Tube, Fig. 3.
5.2.1 Spacers (for metal specimen), of borosilicate glass,
standard wall, 9 mm outside diameter, 6 mm length.
5.2.2 Oil Sampling Tube, Borosilicate Glass, 4 mm outside
Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,
Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098. diameter, with sampling end approximately 600 mm to reach
D5968 − 06 (2013)
FIG. 4 Thermocouple Tube
FIG. 6 Assembled Apparatus
5.3 Other items and equipment are:
5.3.1 Heating Bath, constant temperature control within
60.5 °C (61 °F) of test temperature with an immersion depth
of 23 cm to 35 cm. Oil or aluminum baths are recommended.
(Warning—There are exposed hot surfaces on apparatus.
Avoid skin contact by use of protective equipment.)
5.3.2 Hood Ventilation, to adequately remove fumes during
heating.
5.3.3 Air Supply, use air from a clean, dry source.
5.3.4 Flowmeter, capable of measuring 10 L/h 6 1 L/h.
5.3.5 Balance, analytical sensitivity 0.1 mg.
5.3.6 Balance, Laboratory, 2500 g capacity, 0.1 g sensitiv-
ity.
5.3.7 Microscope, with 20-diameter magnification.
5.3.8 Assembly Fixture, wood slotted to hold coupons
squares (assembly as shown in Fig. 7) for tying with wire.
5.3.9 Whenairneedstobeconditionedthereisaneedforan
air drier. The method used is optional provided the air
characteristics of 5.3.3 are attained. For drying, a satisfactory
FIG. 5 Condenser, Allihn Type
method is the use of a glass column containing 8-mesh
anhydrous calcium sulfate with a column diameter such that
into main sample tube. Tube is bent U-shape with exit end
velocity of air does not exceed 1.2 m/min.
fitted by a one-hole stopper to a 25 mLfiltering flask. Exit end
5.3.10 Oven, optional, to dry glassware at elevated tempera-
may be any convenient length.
ture.
7,8
5.2.3 Adapter, Polytetrafluoroethylene for 10/18 joint for
5.3.11 Forceps, stainless steel.
sealing of air tube to sample tube head.
5.3.12 Thermocouple.
5.3.13 Brush,short-bristled,stiff(old-styletypewriterclean-
ing brush or equivalent).
A satisfactory source for this item is Kontes Glass Co., Vineland, NJ 08360.
The sole source of supply of the apparatus known to the committee at this time
is noted in the adjoining footnote. If you are aware of alternative suppliers, please 6. Reagents and Materials
provide this information to ASTM Headquarters. Your comments will receive
6.1 Purity of Reagents—Use reagent grade chemicals in all
careful consideration at a meeting of the responsible technical committee, which
you may attend. tests.Unlessotherwiseindicated,itisintendedthatallreagents
D5968 − 06 (2013)
6.7 Degreasing Solvents, Trichlorotrifluorethane or 1,1,1-
trichloroethane. (Warning—Harmful if inhaled.)
6.8 Glassware Cleaning Solution, mix 35 mL of saturated
sodium dichromate (aqueous) solution and 1000 mL of con-
centrated sulfuric acid. (Warning—Causes severe burns.)
12,8
6.9 Carbon Remover for Glassware , Oakite Stripper
R-8. (Warning—Corrosive, causes severe burns.)
6.10 Tetrahydrofuran. (Warning—Toxic and flammable.
Health hazard.)
6.11 Naphtha, Aromatic. (Warning—Flammable. Health
hazard.)
6.12 Filter Paper.
6.13 Kimwipe Tissues, or similar.
6.14 Industrial Reference Oil.
7. Preparation of Apparatus
7.1 Cleaning of Glassware from Previous Run:
7.1.1 Rinse all glassware items and the air tube adapter with
degreasing solvent to remove residual oil, and air dry.
(Warning—Harmful if inhaled.)
7.1.2 Fill or immerse the sample tube, air tube, and the
9 mm glass spacers in carbon remover at room temperature
until carbonaceous deposits are removed. Water rinse after
removal. (Warning—Corrosive, causes severe burns.)
FIG. 7 Arrangement of Metal Coupons
7.1.3 Wash all glassware items and the air tube adapter with
13,8
detergent. Rinse with water to remove detergent, and dry.
7.1.4 Store all items in a dust free cabinet until needed for
conform to the specifications of the Committee on Analytical
test. If stored longer than one week, rinse again with distilled
Reagents of the American Chemical Society where such
water before use, and dry.
specifications are available.
7.1.5 A more elaborate glass cleaning procedure can be
10,8
used, if it is for a given situation. This cleaning procedure is
6.2 Metal Specimens:
necessary in a referee situation unless a cleaning solution can
6.2.1 Coupons, 0.081 cm thick by 2.5 cm square, one each,
be used which is satisfactory to all parties involved. Fill and
with two drilled holes (as shown in Fig. 7), as follows:
immerse all glassware items with glassware cleaning solution
6.2.1.1 Copper (R401-A),
and soak for 3 h to 16 h. (Warning—Corrosive, causes severe
6.2.1.2 Lead (R401-lead),
burns.)
6.2.1.3 Tin (R401-tin), and
7.1.6 Remove glassware from cleaning solution, rinse sev-
6.2.1.4 Phosphor Bronze (R401-LEADz).
eral times with tap water, followed by distilled water, and oven
6.3 Nichrome Wire, clean (for tying coupons together).
dry.
6.4 Abrasive Paper, 240 grit aluminum oxide and 400 grit
7.2 Cleaning of Glassware (New):
silicon-carbide. Do not use iron-containing abrasives such as
7.2.1 Proceed as in 7.1.3 and 7.1.6 in that order (omit 7.1.1,
natural emery.
7.1.2, 7.1.4, and 7.1.5).
6.5 Cotton, absorbent.
7.3 Assembly—Assemble as shown in Fig. 6 using only the
6.6 Acetone (ACS), sulfur-free. (Warning—Flammable.
test oil to lubricate glass joints during assembly.
Health hazard.
7.4 Preparation of Metal Specimens:
7.4.1 Wash a length of the metal tying wire with tetrahy-
drofuran and acetone and allow to dry. (Warning—This and
Reagent Chemicals, American Chemical Society Specifications, American
thefollowingpreparationprocessesshouldbeperformedunder
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
listed by the American Chemical Society, see Annual Standards for Laboratory
a fume hood.)
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
7.4.2 The metal squares are prepared as follows:
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD.
Satisfactory metal specimens may be obtained from: Test Engineering, Inc.
(TEI), 12718 Cimarron Path, SanAntonio,TX 78249-3423.This is the only coupon Oakite Stripper R-8 is available from Oakite Products, Inc., 50 Valley Rd.,
source to be used for obtaining a valid reference run and data for certification. Berkeley Heights, NJ 07922. It has been found satisfactory for this purpose.
11 13
Suitable abrasive paper meeting these specifications is included with the metal A detergent found satisfactory is Alconox made by Alconox, Inc., 215 Park
coupons from the source indicated in 6.2. Ave. S., New York, NY 10003.
D5968 − 06 (2013)
7.4.2.1 Usingthe240gritabrasivepaper,removeallsurface Correct the leak, and repeat the determination, using fresh oil
blemishes from both sides and all four edges of each square, sample and new coupons.
and any burrs from the drilled holes. Finish polishing with 400
8.3.4 Using forceps, withdraw the coupons from the test
grit paper wetted by acetone to remove marks from previous tube, and remove the wire holding them together. (Retain the
polishing.Agood technique is to place abrasive paper on a flat
test tube and sample for further examination).
surface, then rub the specimen with longitudinal strokes in a
8.4 Preparing Squares for Examination:
direction perpendicular to that used with 240 grit paper. Use a
8.4.1 Using forceps, wash each square individually in tet-
different sheet of paper for each metal type.
rahydrofuran.
7.4.2.2 In all succeeding steps, handle the squares only with
8.4.2 Repeat the washing, using fresh tetrahydrofuran,
tongs or filter paper until the final weighing. If large defects or
scrubbing the squares with the short-bristled brush until the
particles are present on the metal coupons, course sand paper
tetrahydrofuran shows no additional discoloration. Use a piece
should be used first to remove them; this is followed by
of Kimwipe, dampened with acetone, to rub and wipe the
polishing with the 240 and 400 grit abrasive paper.
coupons repeatedly until the tissue remains clean after wiping.
(1) Store the polished metal coupon in tetrahydrofuran and
Allow the squares to air-dry. The reaction products that are to
proceed until all coupons are polished.
be removed by this cleaning process may tend to have a
(2) Remove each square from the tetrahydrofuran, clean all
stronger affinity to the br
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